Tris [(trimethylsilyl)oxy] antimony

1994 ◽  
Vol 49 (7) ◽  
pp. 855-858 ◽  
Author(s):  
Michael Baier ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Gas Phase ◽  
Structure Determination ◽  
Spectroscopic Data ◽  
Mass Spectrometric ◽  
Unit Cell ◽  
The Other ◽  
X Ray ◽  
Trigonal Bipyramidal

Abstract Tris[(trimethylsilyl)oxy]antimony (Sb(OSiMe3)3, 1) has been prepared from SbCl3 and 3 equiv. of LiOSiMe3 in diethylether. According to mass spectrometric and NMR spectroscopic data, 1 appears to be a monomer in solution and in the gas phase. Dimerisation occurs, however, in the solid state as verified by an X-ray crystal structure determination. The unit cell contains three crystallographically independent monomers, two of which form one type of dimer, while the other is part of a centrosymmetrical dimer. In both types of dimers two Sb atoms are connected via two OSiMe3 groups to form distorted Sb2O2-squares. Together with the remaining 4 OSiMe3 groups and the two stereochemically active lone pairs, each Sb exhibits a trigonal bipyramidal coordination.

Synthesis and Crystal Structure Determination of (R,S)-Diphenyl 1-CyclohexyI-1-(4-nitroanilino)methanephosphonate

1997 ◽  
Vol 52 (12) ◽  
pp. 1544-1548
Author(s):  
Adel Amer ◽  
Ho Hans ◽  
Hans Zimmer
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Gas Phase ◽  
Structure Determination ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Fab Mass Spectrometry ◽  
Long Time

Though diphenyl 1,1-diarylsubstituted phosphonates are known for a long time, FAB-mass spectrometry and X-ray crystal analysis revealed that these species occur as dimers in the solid state and in the gas phase.

Über neue monocyclische Acyloxyfluoroborane 2.2.6.6-Tetrafluoro-1.4-dialkyl-1.3.5-trioxa-1.6-diboracyclohexene: Darstellung, Molekül- und Kristallstruktur/ New Monocyclic Acyloxyfluoroboranes 2,2,6,6-Tetrafluoro-1,4-dialkyl-1,3,5-trioxa-2,6-diboracyclohexenes: Synthesis, Molecular and Crystal Structure

1983 ◽  
Vol 38 (5) ◽  
pp. 554-558 ◽  
Author(s):  
Herbert Binder ◽  
Walter Matheis ◽  
Hans-Jörg Deiseroth ◽  
Han Fu-Son
Keyword(s):  
Crystal Structure ◽  
Organic Acid ◽  
Structure Determination ◽  
Unit Cell ◽  
Ring Conformation ◽  
X Ray ◽  
Conformational Isomers ◽  
Ring Group ◽  
Acid Anhydrides

Abstract Acyloxyfluoroboranes Trimeric alkoxydifluoroboranes (F2BOR)3 (2) react with organic acid anhydrides by substitution of a ring group OR forming monocyclic acyloxyfluoroboranes of the type 2,2,6,6-tetrafluoro-l,4-dialkyl-l,3,5-trioxa-2,6-diboracyclohexene (3). The X-ray crystal structure determination of 3a shows two conformational isomers: two planar and two non-planar six-membered rings are present in the unit cell. The ring conformation is influenced by weak intermolecular H — F interactions.

Synthese und Kristallstruktur des Dichloroselenonitren-Komplexes (PPh4)2[WCl5(NSeCl2)] / Synthesis and Crystal Structure of the Dichloro-selenonitrene Complex (PPh4)2[WCl5(NSeCl2)]

1992 ◽  
Vol 47 (3) ◽  
pp. 301-304 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Determination ◽  
Selenium Atom ◽  
Tungsten Atom ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral

The title compound has been prepared by the reaction o f [WCl4(NSeCl)]2 with PPh4Cl in CH2Cl2 solution. It forms red crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 3856 observed unique reflections, R = 0.073. Lattice dimensions at 25 °C: a = 2266.0(5), b = 1121.0(2), c = 2013.0(4) pm, β = 109.66(3)°. The structure consists o f PPh4+ ions and anions [WCl5(NSeCl2)]2-, in which the tungsten atom is surrounded in a distorted octahedral way by five chlorine atoms and by the nitrogen atom of the (NSeCl2)3- ligand. The W = N = SeCl2 group is characterized by WN and SeN double bonds; the selenium atom has a pseudo trigonal-bipyramidal coordination with the N atom and two lone pairs in equatorial and the chlorine atoms in axial positions.

A New Bis-Tröger's Base: Synthesis, Spectroscopy, Crystal Structure and Isomerization

2006 ◽  
Vol 71 (9) ◽  
pp. 1278-1302 ◽  
Author(s):  
Martin Valík ◽  
Pavel Matějka ◽  
Eberhardt Herdtweck ◽  
Vladimír Král ◽  
Bohumil Dolensky
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Data ◽  
The Other ◽  
X Ray Diffraction ◽  
One Pot ◽  
Molecular Tweezers ◽  
X Ray ◽  
Troger's Base ◽  
Ir And Raman ◽  
C Nmr

A new bis-Tröger's base was prepared from a tetraamine precursor as a mixture of two diastereoisomers. One of the isomers has a chair-like geometry, and the other possesses a boat-like geometry, embodying molecular tweezers. A one-pot preparation of bis-TB isomers and their interconversion under acid conditions was also studied. Structures of both isomers were confirmed by single-crystal X-ray diffraction. Extensive spectroscopic data, including 1H and 13C NMR, IR and Raman spectra of the isomers, are given.

Structural Properties of a Dimeric Phenylcyanamidocopper(I) Complex, [{Cu(PPh3)2(C6H5NCN)}2]

2000 ◽  
Vol 53 (12) ◽  
pp. 971 ◽  
Author(s):  
Eric W. Ainscough ◽  
Andrew M. Brodie ◽  
Peter C. Healy ◽  
Joyce M. Waters
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Properties ◽  
Structure Determination ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
X Ray ◽  
Angle Spinning

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

Organoamido- and Aryloxo-Lanthanoids. XI. Syntheses and Crystal Structures of Nd(Odpp)3, Nd(Odpp)3(thf) and [Nd(Odpp)3(thf)2].2(thf) (Odpp-=2,6-Diphenylphenolate): Variations in Intramolecular π-Ph-Nd Interactions

1995 ◽  
Vol 48 (4) ◽  
pp. 741 ◽  
Author(s):  
GB Deacon ◽  
TC Feng ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Phenyl Group ◽  
Triangular Array ◽  
The Other ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The X-ray crystal structure of Nd (Odpp)3 ( Odpp- = 2,6-diphenylphenolate), obtained by sublimation of Nd ( Odpp )3( thf )2 ( thf = tetrahydrofuran ) [triclinic, Pī , a 15.835(5), b 13.499(10), c 10.955(11) Ǻ, α 116.25(7), β 92.87(7), γ 101.66(6)°, V 2031 Ǻ3, Z2, No 5726 'observed' data (I > 3σ(I)) refined to conventional R 0.047 shows a near triangular array of oxygens surrounding neodymium { Nd -O} 2.169 Ǻ, ∑ O- Nd -O 353.2° with additional, intramolecular Nd-η6-Ph chelate interactions { Nd -C} 3.046 Ǻ and Nd-η1-Ph ( Nd -C 2.964(7)Ǻ). There is a pseudotrigonal bipyramidal arrangement of the oxygens, the centroid of the η6-Ph, and the η1-carbon. The complex Nd ( Odpp )3( thf ), obtained by crystallization of Nd ( Odpp )3( thf )2 from toluene (monoclinic, P21/c, a 12.213(4), b 21.447(4), c 17.744Ǻ, β 104.25(2)°, V 4505 Ǻ3, Z 4, R 0.042 for No 8014) also has pseudotrigonal bipyramidal stereochemistry, with a triangular equatorial array of aryl oxide oxygens { Nd -O} 2.193 Ǻ; ∑ O- Nd -O 358.7°, an apical thf oxygen (Nd -O 2.446(3)Ǻ), and an apical intramolecular chelating phenyl group. As the last has three Nd -C contacts (3.094(5), 3.144(5), 3.010(5)Ǻ) significantly shorter than the other three (3.300(5), 3.427(5), 3.377(5)Ǻ), an η3-Ph-Nd interaction seems likely. For [ Nd ( Odpp )3( thf )2].2( thf ), obtained by crystallization from tetrahydrofuran without drying of the crystals, the X-ray structure (monoclinic, P21, a 10.230(2), b 21.919(5), c 13.411(4) Ǻ, β 101.15(2)°, V 2950 A3, Z2, R 0.058 for No 3237) reveals a distorted trigonal bipyramidal arrangement of three aryl oxide oxygens (two equatorial 2.208(9), 2.16(1) Ǻ; one axial 2.203(9) Ǻ) and two thf oxygens (one equatorial 2.44(1) Ǻ; one axial (significantly distant) 2.62(1) Ǻ). The X-ray structure of [La( Odpp )3( thf )2].2( thf ) shows it to be isostructural with the neodymium analogue.

Study of Garnets by ALCHEMI

2001 ◽  
Vol 7 (S2) ◽  
pp. 358-359
Author(s):  
János L. Lábár ◽  
Lajos Tόth ◽  
István Dόdony ◽  
Jerzy Morgiel
Keyword(s):  
Crystal Structure ◽  
Chemical Composition ◽  
High Sensitivity ◽  
Unit Cell ◽  
Previous Literature ◽  
The Other ◽  
Axial Orientation ◽  
Partial Substitution ◽  
X Ray ◽  
Oxygen Atoms

Garnets were one of the first materials in which an occupation of separate lattice sites by different atomic species was determined with an ALCHEMI technique proposed by Spence and Tafto in l982. The reason of so much interest in this material was twofold, i.e. first its known high sensitivity of X-ray generation depending on orientation especially in the axial orientation and second its complicated crystal structure allowing different atomic arrangements in the unit cell depending on its chemical composition. The dodecahedral (X), octahedral (Y) and tetrahedral (Z) sites between the relatively large oxygen atoms can be filled with a variety of small cations in accordance with the formula X3Y2Z3O12. Partial substitution of one cation with another is common in this structure. The results presented in the previous literature indicated that ALCHEMI can only separate the Y-sites from the sum of the other two (X+Z), while the latter has to remain unresolved.

Notizen: Eine neue bicyclische Zinn-Selen-Verbindung. Synthese und Kristallstruktur von [{Cp(CO)2Fe}3ClSn3Se4] / A New Bicyclic Tin Selenium Compound. Synthesis and Crystal Structure of [{Cp(CO)2Fe}3ClSn3Se4]

1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Selenium Compound ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Compound Synthesis

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.

scholarly journals Metallation of Isatin (2,3-Indolinedione). X-Ray Structure and Solution Behavior of Bis(Isatinato)Mercury(II)

1995 ◽  
Vol 2 (2) ◽  
pp. 81-90 ◽  
Author(s):  
Angel Garcia-Raso ◽  
Juan J. Fiol ◽  
Elies Molins ◽  
Antonia M. Calafat ◽  
Patricia A. Marzilli ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Metal Complex ◽  
Bond Length ◽  
Spectral Data ◽  
Structure Determination ◽  
Monoclinic System ◽  
Heterocyclic Nitrogen ◽  
X Ray

The first X-ray structure of an isatin (2,3-indolinedione, isaH) metal complex, bis(isatinato)memury(II) (C16H8N2O4Hg) (1), was determined. (1) was obtained from the reaction of isaH with mercury(II) acetate in methanol. Analogously, treatment of sodium saccharinate and mercury(II) acetate in methanol yielded Hg(saccharinato)2•0.5CH3OH (3). (1) crystallizes in the monoclinic system, space group P21/a with a = 7.299(1) Å, b = 8.192(1) Å, c = 11.601(1) Å , β = 105.82(1)°, V = 667.4 Å3, Z = 2, Dcalc = 2.452 g cm−3, MoKα radiation(λ = 0.71073 Å), μ = 115.5 cm-1, F(000) = 460, 21(1) °C. The structure was refined on the basis of 2023 observed reflections to R= 0.044. The two deprotonated, non coplanar isa ligands are trans to each other in a head to tail orientation and bound to the Hg through the nitrogen in a linear N-Hg-N arrangement. The Hg atom is at the center of symmetry of the complex and displaced by 0.62 Å from the two planes of the isa ligands (τ Hg-N1-C2-O2= -16°). The Hg-N bond length is 2.015 Å. Noπ-aryl-memury(ll)-π-aryl stacking interaction was observed either in the solid state or in the solution state. The IR, electronic, and H1 and C13NMR spectral data of (1) and (3) suggest binding of the memury to the heterocyclic nitrogen, in agreement with the crystal structure determination of (1).

Organoamido- and Aryloxo-lanthanoids. X. Tris(η2-3,5-di-t-butylpyrazolato)lanthanoid(III) Complexes and the X-Ray Crystal Structure of Er(η2-But2pz)3(thf)2

1994 ◽  
Vol 47 (7) ◽  
pp. 1223 ◽  
Author(s):  
JE Cosgriff ◽  
GB Deacon ◽  
BM Gatehouse ◽  
H Hemling ◽  
H Schumann
Keyword(s):  
Crystal Structure ◽  
Triphenylphosphine Oxide ◽  
The Other ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Oxygen Atoms

The complexes Ln (But2pz)3( thf )2 ( Ln = Y, La, Pr, Nd , Sm, Gd, Dy , Er , Yb, Lu; But2pz- = 3,5-di-t-butylpyrazolate; thf = tetrahydrofuran ), and [ Ln (But2pz)3(OPPh3)2].( dme )n ( Ln = La, n = ⅔ ; Ln = Er , n = 1; dme = 1,2-dimethoxyethane) have been prepared by reaction of the lanthanoid metal with bis ( pentafluorophenyl )mercury and the corresponding pyrazole in either thf , or in dme in the presence of triphenylphosphine oxide. The X-ray crystal structure of Er (η2-But2pz)3( thf )2 [monoclinic, space group P21 (No. 4), a 9.738(4), b 19.602(4), c 11.636(4) Ǻ, β 99.42(3)°, R 0.0374 for 3667 observed reflections] shows the complex to be an eight-coordinate monomer with three chelating But2pz ligands . The arrangement of centres ( Cen ) of the N-N bonds of the But2pz ligands [< Er -N> 2.336 Ǻ; Cen-Er-Cen 140.1(4)°, 110.3(4)° and 109.6(4)°] and the thf oxygen atoms [< Er -O> 2.351 Ǻ; O- Er -O 140.1(4)°] is intermediate between trigonal bipyramidal and square pyramidal. The other Ln (But2pz)3( thf )2 complexes and Ln (But2pz)3(OPPh3)2 are considered to have similar structures.

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